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Structural, spectroscopic and computational studies on the monoclinic polymorph (form I) of potassium hydrogen disilicate (KHSi2O5)

Published online by Cambridge University Press:  05 July 2018

D. Schmidmair ,
V. Kahlenberg ,
L. Perfler  and
D. M. Többens
D. Schmidmair
Affiliation:
Institute of Mineralogy and Petrography, University of Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
V. Kahlenberg*
Affiliation:
Institute of Mineralogy and Petrography, University of Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
L. Perfler
Affiliation:
Institute of Mineralogy and Petrography, University of Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
D. M. Többens
Affiliation:
Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Department of Crystallography, Hahn-Meitner- Platz 1, D-14109 Berlin, Germany
*
E-mail: [email protected]
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Abstract

Hydrothermal treatment of quartz with 2 M K2CO3 solutions at 623 K and 1 kbar resulted in the formation of single crystals of the monoclinic polymorph of potassium hydrogen disilicate (KHSi2O5 or KSi2O4(OH)). Basic crystallographic data of this so-called phase I at room conditions are as follows: space group C2/m, a = 14.5895(10) Å, b = 8.2992(3) Å, c = 9.6866(7) Å, β = 122.756(10)°, V = 986.36(10) Å3, Z = 8. The structure was determined by direct methods and refined to a residual of R(|F|) = 0.0224 for 892 independent observed reflections with I > 2σ(I). The compound belongs to the group of chain silicates. It is based on crankshaft-like vierer double-chains running parallel to [010]. The H atoms are associated with silanol groups. Hydrogen bonding between neighbouring double-chains results in the formation of ∼5 Å wide slabs. The three crystallographically independent K cations with six to eight O ligands provide linkage (1) between the chains of a single slab or (2) between adjacent slabs. Structural investigations have been supplemented by micro-Raman spectroscopy. The interpretation of the spectroscopic data including the allocation of the bands to certain vibrational species has been aided by DFT calculations.

Keywords

KHSi2O5polymorphismsingle-crystal X-ray diffractionstructure refinementRaman spectroscopyDFT calculation
Type
Research Article
Information
Mineralogical Magazine , Volume 78 , Issue 3 , June 2014 , pp. 609 - 622
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2014

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KHSi2O5 RT 293K cif

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KHSi2O5 LT 173K Cif

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